CN109536394B - Preparation method and application of storax extract - Google Patents
Preparation method and application of storax extract Download PDFInfo
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- CN109536394B CN109536394B CN201811332140.3A CN201811332140A CN109536394B CN 109536394 B CN109536394 B CN 109536394B CN 201811332140 A CN201811332140 A CN 201811332140A CN 109536394 B CN109536394 B CN 109536394B
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- storax
- aroma
- extract
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Classifications
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a preparation method and application of storax extract, which adopts tobacco stems and peanut shells as biological materials to adsorb a composite biological preparation, biologically converts residue after resin is squeezed from the bark of the storax, and extracts and prepares the storax extract by a continuous countercurrent ultrasonic extraction technology, so that the storax extract has rich and natural fragrance such as fresh violet, cinnamon, baking aroma, baking cheese aroma and the like, the irritation is reduced, the quality of the spice is improved, the extraction rate is improved, the raw materials are cheap and easy to obtain, and the process conditions are mild; the cigarette is applied to novel cigarettes heated by electricity and carbon, is coordinated with cigarette aroma, enriches aroma, has cinnamon aroma, fresh violet aroma, baking aroma, roasted cheese aroma and the like, reduces irritation, and increases throat comfort.
Description
Technical Field
The invention relates to the field of tobacco additives, in particular to a preparation method and application of a storax extract.
Background
The additive for tobacco is an assistant for improving the physical and chemical properties of tobacco, and comprises spice essence, a humectant, a combustion improver, a mildew preventive and an adsorbent. Compared with the traditional combustion type cigarette, the heating temperature of the non-combustion type cigarette is generally 500 ℃ or less, usually 300 ℃, the action on aroma substances in the cigarette and the mechanism for generating aroma are different, the sensory effect difference with the cigarette smoking is often larger, and the flavoring is needed to make up for the deficiency of the cigarette aroma. The natural perfume meets the requirements of consumers on health better due to natural property, safety and natural compound aroma, but still has the defects of low extraction efficiency, more solvent residues, high impurity content, low purity, high cost caused by complex purification steps, obvious characteristic aroma, additional aroma for covering cigarette aroma and the like. Because most of the perfume materials are compounds with lower molecular weight, low boiling point and stronger volatility, the loss is serious in the high-temperature processing process, so that the phenomenon of nonuniform fragrance release is caused, and the fragrance is lost due to volatilization even in the storage period or the chemical property is unstable and is easy to be oxidized and deteriorated.
Storax is a resin secreted by the liquidambarientalismill of the plant styrax of hamamelidaceae (named as origin, compendium of materia medica, say, "this fragrance is out of the storax" and named as the name "). Also named as Di ointment (Houning Ji's medicine spectra), storax oil (Taiping atlantoau records), storax oil (local prescription), and Di oil stream (modern practical Chinese medicine). Storax is an irritant expectorant, has weak antibacterial effect, and can be used for treating various respiratory tract infections.
The natural extract is prepared by the conventional preparation methods of water extraction, alcohol extraction and the like, and has the defects of increasing irritation, offensive odor and residual feeling while adding protein, tannin, starch, pectin, cellulose, lignin and other macromolecular substances which are not good for cigarette smoking taste while extracting fragrant substances. The biological aroma production technology is a new technology which utilizes biological technologies such as microbial engineering, enzyme engineering, cell culture, gene modification and the like to metabolize specific aroma components through microorganisms so as to improve the quality of products. In the process of preparing natural perfume by biological perfume production technology, suspended microorganism fermentation is mostly adopted, and the mode also has the defects of low yield of natural extract and extractive perfume products, unstable product quality, complex purification steps, high cost and the like, and seriously hinders the application and popularization of biological perfume production natural perfume.
The patent of 'a storax snuff' (patent number ZL201310013441.0) at present discloses a storax snuff made of pure natural raw materials and a preparation method thereof, the storax snuff is composed of 6-14 parts (by weight) of natural raw materials containing storax, and the storax snuff can refresh the mind, refresh the brain, ventilate the nasal cavity and assist in quitting smoking; the patent of 'storax extract for cigarette and its preparation method' (patent number ZL201510173828.1) discloses a preparation method: crushing dried storax, adding the crushed storax, fructose and acetic acid into 70-95% ethanol solution, soaking, heating, refluxing and extracting for 2-5h, cooling, filtering and concentrating to obtain storax extract, wherein the storax extract is applied to cigarettes to ensure that the cigarettes have rich fragrance, strong sweet taste, low dry feeling of smoke, weak spicy feeling and irritation, and the harmful components benzo [ a ] pyrene and phenol in the smoke are obviously reduced; the patent 'preparation method and application of storax extract for cigarette' (application No. 201210293385.6), soaking storax in aqueous solution containing lactic acid for 1 hour, extracting under heating and refluxing for 3 times under normal pressure, combining three filtrates, concentrating under reduced pressure at 60 deg.C to 2 times of original weight of storax, and applying storax extract to tobacco to improve tobacco fragrance, reduce irritation, and improve throat comfort.
The residue after the resin is squeezed from the styrax bark is used as a raw material, a tobacco stem and peanut shell composite biological material is adopted to adsorb a biological agent, hydrolysis fermentation pretreatment is carried out, then, a styrax extract is obtained through a continuous countercurrent ultrasonic extraction technology, and the styrax extract is applied to novel cigarettes heated by electricity and carbon, and has the effects of enriching aroma, reducing irritation, relieving cough and eliminating phlegm and enhancing throat comfort.
Disclosure of Invention
According to the defects, the invention aims to provide a preparation method and application of a storax extract, wherein a tobacco stem and peanut shell biological material are adopted to adsorb a composite biological agent, residues after resin is squeezed from the bark of the storax are biologically converted, and the storax extract is prepared by extracting through a continuous countercurrent ultrasonic extraction technology, so that the storax extract has rich and natural fragrance such as fresh violet, cinnamon, baking aroma, baking cream aroma and the like, the irritation is reduced, the quality of the spice is improved, the extraction rate is improved, the raw materials are cheap and easy to obtain, and the process conditions are mild; the cigarette is applied to novel cigarettes heated by electricity and carbon, is coordinated with cigarette aroma, enriches aroma, has cinnamon aroma, fresh violet aroma, baking aroma, roasted cheese aroma and the like, reduces irritation, and increases throat comfort.
The invention is realized by the following technical scheme:
a method for preparing storax extract comprises the following steps:
(1) pretreatment of raw materials: the residue after the resin is squeezed from the styrax bark is crushed into 40-120 meshes of powder by a crusher;
(2) activation of microbial strains: adding active solid freeze-dried powder of saccharomyces cerevisiae (Saccharomyces fibuligera) and Bacillus methanovorus (VJ4-1) into 5-20 times of sterilized glucose or fructose solution with the mass concentration of 5-30%, and placing the solution in a water bath kettle at 30-45 ℃ for activation for 30-60 min to obtain a microbial strain activation solution, wherein the preservation number of the Bacillus methanovorus (VJ4-1) is CCTCC NO: 2012004, classified and named as Bacillus methylotrophicus (VJ4-1), deposited in China center for type culture Collection of Wuhan university at 1 month and 11 days 2012;
(3) preparing an immobilized carrier: cleaning tobacco stems and peanut shells, drying, processing the tobacco stems into fragments with the length of about 1cm, mixing the fragments with the peanut shells according to a certain proportion, sterilizing at high pressure, and drying to obtain an immobilized carrier;
(4) immobilization treatment of biological agent: putting a certain amount of the immobilized carrier sterilized and dried in the step (3) into a microfiltration bag, putting the microfiltration bag into a container, adding the cultured activation solution and a certain amount of alpha-L-arabinofuranosidase according to the mass ratio of the immobilized carrier to the activation solution of the microbial strain of 1: 1-10, uniformly mixing, and placing the mixture in a refrigerated cabinet at the temperature of 4 +/-0.5 ℃ for fixing for 12-72 hours to obtain a biological agent-immobilized carrier;
(5) adsorption hydrolysis fermentation: uniformly mixing the storax bark residue powder obtained in the step (1) with water of which the mass is 5-15 times that of the storax bark residue powder, adding the mixture into the microporous filter bag filled with the biological agent-immobilized carrier in the step (4), uniformly stirring at 35-65 ℃ at a mass ratio of 1: 2.1-4, adding citric acid to adjust the pH value to be 4.0-6.0, fermenting for 1-6 days, taking out the microporous filter bag, and performing suction filtration to obtain storax fermentation liquor A and storax residue;
(6) feeding the storax residue obtained in the step (5) into a leaching cabin at a speed of 0.1-1.0 kg/10min, starting a main machine and an ultrasonic generator, adjusting the temperature to 60-98 ℃, the material-liquid ratio to be 1: 2-10 by mass, adding potassium hydroxide, uniformly stirring, adjusting the pH value to 7-14, operating for 0.2-1 h from the lower end of the leaching cabin, adjusting a liquid outlet valve to uniformly discharge liquid, controlling the adding flow of a solvent, keeping the liquid level of the leaching cabin balanced, feeding barium hydroxide and compound amino acid in a certain proportion when continuous countercurrent ultrasonic extraction reaches 30-60 min, stopping the production process when the continuous countercurrent ultrasonic extraction reaches 90-150 min, and discharging residues to obtain storax B;
(7) liquid-liquid extraction: mixing the storax fermentation liquor A and the leaching solution B in the steps (5) and (6), adding ethyl acetate with the mass 1-15 times that of the storax bark residue powder, heating and refluxing for 2-6 h at 45-65 ℃, carrying out vacuum filtration to retain filtrate, concentrating volatile solvent under reduced pressure at 45-55 ℃ to obtain storax extract, and adding propylene glycol with the mass ratio of 1: 0.5-3 to obtain the storax extract.
Further, the saccharomyces cerevisiae and the Bacillus methylotrophicus (VJ4-1) in the step (2) are both food-grade, the vitality is 10-30 u/mg respectively, and the glucose and the fructose are food-grade.
Further, the mass ratio of the tobacco stems to the peanut shells in the step (3) is 1: 0.5-2.
Further, in the step (4), the alpha-L-arabinofuranosidase is food-grade, the enzyme activity is 100-2000 u/g, and the mass ratio of the alpha-L-arabinofuranosidase to the composite active solid freeze-dried bacterial powder in the step (2) is 1: 0.5-2.
Further, the citric acid in the step (5) is food grade, and the rotation speed of uniform stirring is 20-80 rpm.
Further, the ethyl acetate in the step (7) is food grade.
Further, the potassium hydroxide and the barium hydroxide in the step (6) are of analytical pure grade, and respectively account for 0.01-0.2% and 0.1-1% of the mass of the residue powder after the resin is squeezed from the styrax bark.
Further, the compound amino acid in the step (6) is phenylalanine, isoleucine,
Threonine is in food grade, and the mass ratio of threonine to threonine is 1: 0.5-2.
Further, the relative density of the storax extract in the step (7) is 1.0-1.2.
The invention also provides an application of the styrax extract prepared by the method in electrically heating or carbon heating novel tobacco, for example, the styrax extract is added into electrically heating novel tobacco cigarette paper, carbon heating novel tobacco shreds or carbon heating novel tobacco filter sticks according to the mass ratio of 0.1-10 ppm.
The invention has the advantages that:
(1) the tobacco stem and the peanut shell are used as carriers for adsorption and immobilization of the composite biological agent, wherein the tobacco stem is a tobacco original substance and contains strong cellulose adsorption effect, and the peanut shell mainly contains cellulose and phenol-sugar acid polymers, also has the effect of astringing lung and relieving cough, and has rich medicinal value. After the two are mixed according to a certain proportion, the adsorption of the synergistic adsorption microorganism strains and enzymes is strong, the efficiency is high, the desorption is not easy, the cost is low and the biological agent-immobilized carrier is easy to filter and separate from the fermentation liquid;
(2) the residue of the storax bark after the resin is squeezed still contains a large amount of aroma substances and other active ingredients, when the residue is dissolved in water, the residue is incubated, hydrolyzed and fermented under an acidic condition with a complex enzyme system of a biological agent adsorbed on the composite immobilized carrier of the tobacco stems and the peanut shells, the biological aroma production effect is good, and the residue is easy to separate from the strains. The saccharomyces cerevisiae fibuligera has the characteristics of producing amylase, beta-glucosidase, acid protease and the like, can efficiently degrade free cellulose, starch, cellobiose, cane sugar and other macromolecular substances in cell walls of storax residue powder, converts the macromolecular substances into glucose, further converts the macromolecular substances into ester-fragrance-based fragrant substances and ethanol, increases fresh wine fragrance, converts non-volatile glucoside into volatile fragrant substances, produces fragrance, produces ester, removes foreign flavor, destroys cell walls, releases more active chemical substances in cells, improves yield and increases natural complexity of fragrance; bacillus methylotrophicus (VJ4-1) has the capability of producing beta-galactosidase activity to convert non-volatile glucoside into volatile aroma substances, convert cell walls and free ferulic acid to synthesize natural vanillin, and can decompose and utilize saccharides such as glucose, sucrose, rhamnose, maltose, turanose, trehalose to produce aroma components such as alcohol, ester and acid, so that the storax residue fermentation liquor contains milk aroma components such as vanillin and aroma precursor thereof, the cell walls are damaged to release more effective components, and the extraction rate is improved. The alpha-L-arabinofuranosidase acts on 6-O-beta-L-arabinofurano-beta-D-pyranoside to break the disaccharide connection between disaccharide glycosides to generate alpha-L-arabinofuranose and beta-D-pyranoside respectively, which generate glucose and corresponding glycosyl groups under the action of beta-glucosidase activity of Saccharomyces cerevisiae to release bonded aromatic substances, and the two-step glycoside hydrolysis mode enables the storax residue to generate more abundant aroma components. Under the synergistic and strong combined action of the microbial aroma-producing strain and glycosidase, the non-volatile glycoside is better converted into volatile aroma components, cellulose, cellobiose and ferulic acid in cell walls are more effectively decomposed to release intracellular active components, polysaccharide substances are degraded into volatile aroma-causing small molecular components, part of glucose can be converted into ethanol and released into fermentation liquor, and the fermentation liquor is naturally compounded with rich fresh flower aroma, milk aroma, meat sweet-scented osmanthus and lemon aroma and can be separated from an immobilized carrier with the microbial strain through simple filtration, so that the steps are simple;
(3) and then continuous countercurrent ultrasonic extraction and compound amino acid Maillard color-enhancing and aroma-enhancing reaction are combined under the alkaline condition to ensure that the species of the storax extract are richer, more water-soluble protein, cellulose, pectin and other macromolecular irritant impurities are removed by liquid-liquid extraction, barium hydroxide is added in the extraction process to further adsorb the residual impurities which influence the odor absorption in the fermentation liquor, such as tannin components, further enhance the aroma and reduce the impurities, the storax extract is obtained by removing the solvent by concentration under reduced pressure, propylene glycol is added to dilute and dissolve the storax extract into the storax extract which is suitable for heating and non-combustion, and the storax extract has rich and natural aromas such as fresh violet, cinnamon, baking aroma, baking cream aroma and the like, the irritation is reduced, the quality of the spice is improved, the process condition is mild, the production time is short, and more aroma components are extracted as much as.
In general, the method of the invention enables the impurity macromolecule components in the residue after the resin is squeezed from the storax to be decomposed and converted into fragrant substances including protein, cellulose, polysaccharide, starch and the like, reduces impurity foreign flavor, reduces irritation, increases natural complexity of fragrance types, has rich and natural fragrance of fresh flower fragrance, milk fragrance, cassia oil, cinnamon fragrance, mild spicy fragrance, lemon fragrance and the like, reduces irritation, and improves fragrance quality; the production process has mild conditions, simple steps, easy operation and high extraction rate; according to the mass ratio of 0.1-10 ppm, the flavoring agent is applied to electrically heated or carbon heated novel tobacco, is coordinated with tobacco fragrance, enriches fragrance, has fresh violet fragrance, cinnamon fragrance, baking fragrance, cheese baking fragrance and the like, reduces irritation, and increases throat comfort.
Detailed Description
The following specific examples illustrate the present invention in detail.
Example 1
A method for preparing storax extract comprises the following steps:
(1) pretreatment of raw materials: squeezing storax bark to obtain resin residue, and pulverizing into 40 mesh powder;
(2) activation of microbial strains: adding active solid freeze-dried powder of saccharomyces cerevisiae (Saccharomyces fibuligera) and Bacillus methanovorus (VJ4-1) into 5-time sterilized glucose solution with mass concentration of 5%, and placing the glucose solution in a water bath kettle at 30 ℃ for activation for 30min to obtain a microbial strain activation solution, wherein the preservation number of the Bacillus methanovorus (VJ4-1) is CCTCC NO: 2012004, deposited at the China center for type culture Collection of Wuhan university at 11/1/2012;
(3) preparing an immobilized carrier: cleaning tobacco stems and peanut shells, drying, processing the tobacco stems into fragments with the length of about 1cm, mixing the fragments with the peanut shells according to the mass ratio of 1:0.5, and drying after autoclaving to obtain immobilized carriers;
(4) immobilization treatment of biological agent: putting a certain amount of the immobilized carrier sterilized and dried in the step (3) into a microfiltration bag, putting the microfiltration bag into a container, adding the cultured activation solution and a certain amount of alpha-L-arabinofuranosidase according to the mass ratio of the immobilized carrier to the activation solution of the microbial strain of 1:1, uniformly mixing, and placing the mixture in a refrigerated cabinet at the temperature of 4 +/-0.5 ℃ for fixation for 12 hours to obtain a biological agent-immobilized carrier;
(5) adsorption hydrolysis fermentation: uniformly mixing the storax bark residue powder obtained in the step (1) with 5 times of water by mass, adding the mixture into the microporous filter bag filled with the biological agent-immobilized carrier in the step (4), uniformly stirring at 35 ℃ and a constant speed, adding citric acid to adjust the pH value to be 4.0, fermenting for 1d, taking out the microporous filter bag, and performing suction filtration to obtain storax fermentation liquor A and storax residue;
(6) feeding storax residues obtained in the step (5) into a leaching cabin at a speed of 0.1kg/10min, starting a main machine and an ultrasonic generator, adjusting the temperature to 60 ℃ and the material-liquid ratio to be 1:2, adding potassium hydroxide, uniformly stirring, adjusting the pH value to 7, operating for 0.2h from the lower end of the leaching cabin, adjusting a liquid outlet valve to uniformly discharge liquid, controlling the adding flow of a solvent, keeping the liquid level of the leaching cabin balanced, feeding barium hydroxide and compound amino acid in a certain proportion when continuous countercurrent ultrasonic extraction reaches 30min, stopping the production process when the continuous countercurrent ultrasonic extraction reaches 90min, and discharging residues to obtain storax leachate B;
(7) liquid-liquid extraction: mixing the storax fermentation liquor A and the leaching solution B in the steps (5) and (6), adding ethyl acetate with the mass of 1 time of that of the storax bark residue powder, heating and refluxing for 2 hours at 45 ℃, carrying out vacuum filtration to retain filtrate, carrying out vacuum concentration on volatile solvent at 45 ℃ to obtain storax extract, and adding propylene glycol with the mass ratio of 1:0.5 to obtain the storax extract.
Further, the saccharomyces cerevisiae (saccharomyces fibuligera) and the Bacillus methanotrophic (VJ4-1) in the step (2) are both food grade, the vitality is 10u/mg respectively, and the glucose is food grade;
further, in the step (4), the alpha-L-arabinofuranosidase is food grade, the enzyme activity is 100u/g, and the mass ratio of the alpha-L-arabinofuranosidase to the composite active solid freeze-dried bacterial powder in the step (2) is 1: 0.5.
Further, the citric acid in the step (5) is food grade, and the rotation speed of uniform stirring is 20 rpm.
Further, the ethyl acetate in the step (7) is food grade.
Further, the potassium hydroxide and the barium hydroxide in the step (6) are analytical pure grades, and respectively account for 0.01 percent and 0.1 percent of the mass of the residue powder after the resin is squeezed from the styrax bark.
Further, the compound amino acid in the step (6) is phenylalanine, isoleucine and threonine, and is food grade, and the mass ratio of the three is 1:0.5: 0.5.
Further, the relative density of the storax extract in the step (7) is 1.02.
The invention also provides a storax extract prepared by the method, and the storax extract is added into the novel electric heating tobacco cigarette paper according to the mass ratio of 0.1ppm, so that the cigarette paper has fresh violet aroma and roasted cheese aroma, and is rich in aroma during smoking and has fresh flower aroma and roasted aroma.
Example 2
A method for preparing storax extract comprises the following steps:
(1) pretreatment of raw materials: squeezing storax bark to obtain resin residue, and pulverizing into 80 mesh powder;
(2) activation of microbial strains: adding active solid freeze-dried powder of saccharomyces cerevisiae (Saccharomyces fibuligera) and Bacillus methanovorus (VJ4-1) into fructose solution with the mass concentration of 18% and subjected to sterilization treatment by 12 times, and placing the fructose solution in a water bath kettle at 38 ℃ for activation for 45min to obtain a microbial strain activation solution, wherein the preservation number of the Bacillus methanovorus (VJ4-1) is CCTCC NO: 2012004, deposited at the China center for type culture Collection of Wuhan university at 11/1/2012;
(3) preparing an immobilized carrier: cleaning and drying tobacco stems and peanut shells, processing the tobacco stems into fragments with the length of about 1cm, mixing the fragments with the peanut shells according to the mass ratio of 1:1, and drying after autoclaving to obtain immobilized carriers;
(4) immobilization treatment of biological agent: putting a certain amount of the immobilized carrier sterilized and dried in the step (3) into a microfiltration bag, putting the microfiltration bag into a container, adding the cultured activation solution and a certain amount of alpha-L-arabinofuranosidase according to the mass ratio of the immobilized carrier to the activation solution of the microbial strain of 1:6, uniformly mixing, and placing the mixture in a refrigerated cabinet at the temperature of 4 +/-0.5 ℃ for fixation for 48 hours to obtain a biological agent-immobilized carrier;
(5) adsorption hydrolysis fermentation: uniformly mixing the storax bark residue powder obtained in the step (1) with water of which the mass is 5-15 times that of the storax bark residue powder, adding the mixture into the microporous filter bag filled with the biological agent-immobilized carrier in the step (4), uniformly stirring at 50 ℃, adding citric acid to adjust the pH value to be 5.0, fermenting for 3d, taking out the microporous filter bag, and performing suction filtration to obtain storax fermentation liquor A and storax residue, wherein the mass ratio of the biological agent-immobilized carrier to the storax bark residue powder is 1: 3.2;
(6) feeding storax residues obtained in the step (5) into a leaching cabin at a speed of 0.5kg/10min, starting a main machine and an ultrasonic generator, adjusting the temperature to 75 ℃ and the material-liquid ratio to be 1:6, adding potassium hydroxide, uniformly stirring, adjusting the pH value to 10, operating for 0.6h from the lower end of the leaching cabin, adjusting a liquid outlet valve to uniformly discharge liquid, controlling the adding flow of a solvent, keeping the liquid level of the leaching cabin balanced, feeding barium hydroxide and compound amino acid in a certain proportion when continuous countercurrent ultrasonic extraction reaches 45min, stopping the production process when the continuous countercurrent ultrasonic extraction reaches 125min, and discharging residues to obtain storax leachate B;
(7) liquid-liquid extraction: mixing the storax fermentation liquor A and the leaching solution B in the steps (5) and (6), adding ethyl acetate with the mass 8 times that of the storax bark residue powder, heating and refluxing for 4.5h at 55 ℃, carrying out vacuum filtration to retain filtrate, carrying out vacuum concentration on the volatile solvent at 48 ℃ to obtain storax extract, and adding propylene glycol with the mass ratio of 1:1.8 to obtain the storax extract.
Further, the saccharomyces cerevisiae (saccharomyces fibuligera) and the Bacillus methanotrophic (VJ4-1) in the step (2) are both food grade, the vitality is 20u/mg respectively, and the fructose is food grade;
further, in the step (4), the alpha-L-arabinofuranosidase is food-grade, the enzyme activity is 1200u/g, and the mass ratio of the alpha-L-arabinofuranosidase to the composite active solid freeze-dried bacterial powder in the step (2) is 1: 1.2.
Further, the citric acid in the step (5) is food grade, and the rotation speed of uniform stirring is 55 rpm.
Further, the ethyl acetate in the step (7) is food grade.
Further, the potassium hydroxide and the barium hydroxide in the step (6) are analytical pure grades, and respectively account for 0.1 percent and 0.5 percent of the mass of the residue powder after the resin is squeezed from the styrax bark.
Further, the compound amino acid in the step (6) is phenylalanine, isoleucine and threonine, and is food grade, and the mass ratio of the three is 1:1.2: 1.5.
Further, the relative density of the storax extract in the step (7) is 1.15.
The invention also provides a storax extract prepared by the method, which is applied to carbon-heated novel tobacco shreds according to the mass ratio of 0.3ppm, has rich and full aroma during smoking, and has fresh violet aroma, cinnamon aroma and roasted cheese aroma.
Example 3
A method for preparing storax extract comprises the following steps:
(1) pretreatment of raw materials: squeezing storax bark to obtain resin residue, and pulverizing into 120 mesh powder;
(2) activation of microbial strains: adding active solid freeze-dried powder of saccharomyces cerevisiae (Saccharomyces fibuligera) and Bacillus methanovorus (VJ4-1) into a glucose solution with the mass concentration of 30% and subjected to sterilization treatment by 20 times, and placing the glucose solution in a water bath kettle at 45 ℃ for activation for 60min to obtain a microbial strain activation solution, wherein the preservation number of the Bacillus methanovorus (VJ4-1) is CCTCC NO: 2012004, deposited at the China center for type culture Collection of Wuhan university at 11/1/2012;
(3) preparing an immobilized carrier: cleaning and drying tobacco stems and peanut shells, processing the tobacco stems into fragments with the length of about 1cm, mixing the fragments with the peanut shells according to the mass ratio of 1:2, and drying after autoclaving to obtain immobilized carriers;
(4) immobilization treatment of biological agent: putting a certain amount of the immobilized carrier sterilized and dried in the step (3) into a microfiltration bag, putting the microfiltration bag into a container, adding the cultured activation solution and a certain amount of alpha-L-arabinofuranosidase according to the mass ratio of the immobilized carrier to the activation solution of the microbial strain of 1:10, uniformly mixing, and placing the mixture in a refrigerated cabinet at the temperature of 4 +/-0.5 ℃ for fixing for 72 hours to obtain a biological agent-immobilized carrier;
(5) adsorption hydrolysis fermentation: uniformly mixing the storax bark residue powder obtained in the step (1) with 15 times of water by mass, adding the mixture into the microporous filter bag filled with the biological agent-immobilized carrier in the step (4), uniformly stirring at 65 ℃ with the mass ratio of the biological agent-immobilized carrier to the storax bark residue powder being 1:4, adding citric acid to adjust the pH value to be 6.0, fermenting for 6d, taking out the microporous filter bag, and performing suction filtration to obtain storax fermentation liquor A and storax residue;
(6) feeding storax residues obtained in the step (5) into a leaching cabin at a speed of 1.0kg/10min, starting a main machine and an ultrasonic generator, adjusting the temperature to 98 ℃ and the material-liquid ratio to be 1:10, adding potassium hydroxide, uniformly stirring, adjusting the pH value to 14, operating for 1h from the lower end of the leaching cabin, adjusting a liquid outlet valve to uniformly discharge liquid, controlling the adding flow of a solvent, keeping the liquid level of the leaching cabin balanced, feeding barium hydroxide and compound amino acid in a certain proportion when continuous countercurrent ultrasonic extraction reaches 60min, stopping the production process when the continuous countercurrent ultrasonic extraction reaches 150min, and discharging residues to obtain storax leachate B;
(7) liquid-liquid extraction: mixing the storax fermentation liquor A and the leaching solution B in the steps (5) and (6), adding ethyl acetate 15 times of the mass of the storax bark residue powder, heating and refluxing for 6 hours at 65 ℃, carrying out vacuum filtration to retain filtrate, carrying out vacuum concentration on volatile solvent at 55 ℃ to obtain storax extract, and adding propylene glycol in a mass ratio of 1:3 to obtain the storax extract.
Further, the saccharomyces cerevisiae (saccharomyces fibuligera) and the Bacillus methanotrophic (VJ4-1) in the step (2) are both food grade, the vitality is 30u/mg respectively, and the glucose is food grade;
further, the alpha-L-arabinofuranosidase in the step (4) is food grade, the enzyme activity is 2000u/g, and the mass ratio of the alpha-L-arabinofuranosidase to the composite active solid freeze-dried bacterial powder in the step (2) is 1:2.
Further, the citric acid in the step (5) is food grade, and the rotation speed of uniform stirring is 80 rpm.
Further, the ethyl acetate in the step (7) is food grade.
Further, the potassium hydroxide and the barium hydroxide in the step (6) are analytical pure grades, and respectively account for 0.2 percent and 1 percent of the mass of the residue powder after the resin is extracted from the styrax bark.
Further, the compound amino acid in the step (6) is phenylalanine, isoleucine and threonine, and is food grade, and the mass ratio of the three is 1:2: 2.
Further, the relative density of the storax extract in the step (7) is 1.2.
The invention also provides an application of the storax extract prepared by the method in perfuming a novel carbon-heated tobacco filter stick according to the mass ratio of 10ppm, and the storax extract has fresh violet aroma, fruit aroma and roasted cheese aroma during smoking.
Test example 1: comparative evaluation of sensory Effect of applications
Sensory evaluation comparative experiments were conducted using the styrax extracts prepared in examples 1-3 and a blank control in the electric heating or carbon heating of a new type of tobacco.
The results show (as shown in table 1): the storax extract prepared by the invention is applied to adding aroma in novel tobacco heated by electricity or carbon, the tobacco aroma is coordinated, and the storax extract has rich aromas such as fresh violet aroma, cinnamon aroma, roasted cheese aroma and roasted aroma, the irritation is reduced, and the mouthfeel is improved.
TABLE 1 sensory comparative evaluation of storax extract application
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A preparation method of storax extract is characterized by comprising the following steps:
(1) pretreatment of raw materials: squeezing resin from storax bark to obtain residue, and crushing the residue to powder of 40-120 meshes by using a crusher;
(2) activation of microbial strains: adding active solid freeze-dried powder of saccharomyces cerevisiae (Saccharomyces fibuligera) and Bacillus methanovorus (Bacillus methylotrophicus) VJ4-1 into 5-20 times of sterilized glucose or fructose solution with the mass concentration of 5-30%, and placing the solution in a water bath kettle at the temperature of 30-45 ℃ for activation for 30-60 min to obtain a microbial strain activation solution, wherein the preservation number of the Bacillus methanovorus (Bacillus methylotrophicus) VJ4-1 is CCTCC NO: 2012004, deposited at the China center for type culture Collection of Wuhan university at 11/1/2012;
(3) preparing an immobilized carrier: cleaning and drying tobacco stems and peanut shells, processing the tobacco stems into fragments with the length of about 1cm, mixing the fragments with the peanut shells according to the mass ratio of 1: 0.5-2, and drying after high-pressure sterilization to obtain an immobilized carrier;
(4) immobilization treatment of biological agent: putting a certain amount of the immobilized carrier sterilized and dried in the step (3) into a microfiltration bag, putting the microfiltration bag into a container, adding the cultured activation solution and a certain amount of alpha-L-arabinofuranosidase according to the mass ratio of the immobilized carrier to the activation solution of the microbial strain of 1: 1-10, uniformly mixing, and placing the mixture in a refrigerated cabinet at 4+0.5 ℃ for fixation for 12-72 hours to obtain a biological agent-immobilized carrier;
(5) adsorption hydrolysis fermentation: uniformly mixing the storax bark residue powder obtained in the step (1) with water of which the mass is 5-15 times that of the storax bark residue powder, adding the mixture into the microporous filter bag filled with the biological agent-immobilized carrier in the step (4), uniformly stirring at 35-65 ℃ at a mass ratio of 1: 2.1-4, adding citric acid to adjust the pH value to be 4.0-6.0, fermenting for 1-6 days, taking out the microporous filter bag, and performing suction filtration to obtain storax fermentation liquor A and storax residue;
(6) feeding the storax residue obtained in the step (5) into a leaching cabin at a speed of 0.1-1.0 kg/10min, starting a main machine and an ultrasonic generator, adjusting the temperature to 60-98 ℃, the material-liquid ratio to be 1: 2-10 by mass, adding potassium hydroxide, uniformly stirring, adjusting the pH value to 7-14, operating for 0.2-1 h from the lower end of the leaching cabin, adjusting a liquid outlet valve to uniformly discharge liquid, controlling the adding flow of a solvent, keeping the liquid level of the leaching cabin balanced, feeding barium hydroxide and compound amino acid in a certain proportion when continuous countercurrent ultrasonic extraction reaches 30-60 min, stopping the production process when the continuous countercurrent ultrasonic extraction reaches 90-150 min, and discharging residues to obtain storax B;
(7) liquid-liquid extraction: mixing the storax fermentation liquor A and the leaching solution B in the steps (5) and (6), adding ethyl acetate with the mass 1-15 times that of the storax bark residue powder, heating and refluxing for 2-6 h at 45-65 ℃, carrying out vacuum filtration to retain filtrate, concentrating volatile solvent at 45-55 ℃ under reduced pressure to obtain storax extract, and adding propylene glycol with the mass ratio of 1: 0.5-3 to obtain storax extract;
in the step (4), the alpha-L-arabinofuranosidase is food-grade, the enzyme activity is 100-2000 mu/g, and the mass ratio of the alpha-L-arabinofuranosidase to the active solid freeze-dried powder in the step (2) is 1: 0.5-2;
the compound amino acid in the step (6) is phenylalanine, isoleucine and threonine, and is food-grade, and the mass ratio of the compound amino acid to the compound amino acid is 1: 0.5-2;
the potassium hydroxide and the barium hydroxide in the step (6) are of analytical pure grade, and respectively account for 0.01-0.2% and 0.1-1% of the mass of the residue powder after the resin is squeezed from the styrax bark.
2. A method of preparing a storax extract according to claim 1, wherein: the saccharomyces cerevisiae (Saccharomyces cerevisiae) and the Bacillus methanotrophic VJ4-1 in the step (2) are both food grade, the activities are respectively 10-30 mu/mg, and the glucose and the fructose are food grade.
3. A method of preparing a storax extract according to claim 1, wherein: and (5) the citric acid in the step (5) is food grade, and the rotating speed of uniform stirring is 20-80 rpm.
4. A method of preparing a storax extract according to claim 1, wherein: the ethyl acetate in the step (7) is food grade.
5. A method of preparing a storax extract according to claim 1, wherein: the relative density of the storax extract in the step (7) is 1.02-1.2.
6. The application of the storax extract prepared by the method of any one of claims 1-5 in electrically heated or carbon-heated tobacco is added into electrically heated tobacco cigarette paper, carbon-heated tobacco shreds or carbon-heated tobacco filter sticks according to the mass ratio of 0.1-10 ppm.
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